US3998719A - Isotachophoretic columns - Google Patents

Isotachophoretic columns Download PDF

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Publication number
US3998719A
US3998719A US05/606,574 US60657475A US3998719A US 3998719 A US3998719 A US 3998719A US 60657475 A US60657475 A US 60657475A US 3998719 A US3998719 A US 3998719A
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Prior art keywords
capillary
column
test sample
ions
chambers
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Expired - Lifetime
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US05/606,574
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English (en)
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Mirko Deml
Petr Bocek
Jaroslav Janak
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Czech Academy of Sciences CAS
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Czech Academy of Sciences CAS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/447—Systems using electrophoresis

Definitions

  • the invention relates to isotachophoretic columns for the ionic analysis of a test sample.
  • a pair of reservoirs or chambers that respectively hold diverse types of electrolytes are selectively connected to opposite ends of a capillary tube which is generally wound around a metallic cylinder for thermostatic purposes.
  • the introduction of a test sample into the capillary in the presence of communication between the electrolyte chambers and the ends of the capillary is effective, when a high voltage is applied between electrodes positioned in the electrolyte chambers, to cause a discrete migration of the separate types of ions in the test sample through the capillary in succession in one direction.
  • a suitable detecting device coupled to the ionic flow through the capillary records the pulse-like transition in signal level indicative of the passage of the successive ion types past the measuring point and conveys such signals to a suitable recording device to form an isotachophoregram.
  • the amplitude of the applied electrical voltage, and thereby the speed and efficiency of the ionic separation is limited in such present designs because of the relatively poor electrical insulation that naturally results by interconnecting, via deformable and dimensionally unstable components, the separable subassemblies of the known types of isotachophoretic columns.
  • the column is formed from a unitary insulating block, which includes spaced portions defining the leading and lagging electrode chambers, the passages interconnecting the chambers with the opposite ends of the capillary, and the passage for injecting the test sample into the capillary.
  • the capillary itself is formed with a planar profile, with at least one of its parallel boundary walls being defined by a region of the unitary block.
  • the other wall of the capillary is either a second region of the block itself, or one surface of a separate insulating body that is attached to the main block and that is provided, if desired, with suitable cooling facilities for the capillary.
  • the lonitudinal axis of the planar capillary may illustratively form a linear path within the body, or, alternatively, may be curved into a sinuous or spiral path.
  • the detecting arrangement for the separated ions may include an additional pair of passages formed in the main block and extending from a pair of electrodes to the interior of the capillary at a point intermediate its ends.
  • the resulting unitary, non-deformable and dimensionally stable assembly of the isotachophoretic column leads to an efficient and rapid ionic separation and measurement, and typically reduces the time for the measurement form 30-100 minutes to about 5 minutes.
  • FIG. 1 is an elevation view, in section, of an improved type of composite isotachophoretic column constructed in accordance with the invention.
  • FIG. 2 is a pictorial representation of a typical isotachophoregram obtainable with the arrangement of FIG. 1.
  • the improved isotachophoretic column of the invention employs spaced portions of a unitary insulating block 1 to define the various major subassemblies of the column.
  • a unitary insulating block 1 which may illustratively be formed from an organic glass, includes a pair of spaced upper cylinders 11, 12, which form conventional reservoirs or electrode chambers that are individually associated with lagging and leading electrolytes in a conventional manner.
  • a pair of electrodes 18, 19 are conventionally positioned in the electrode chambers 11 and 12, and are connected across a high voltage source 26.
  • the electrode 18 associated with the lagging electrolyte is poled as a cathode, while the electrode 19 associated with the leading electrolyte is poled as an anode.
  • the terms “leading” and “lagging,” as applied to the electrolytes in the chambers 11 and 12, refer to the relative times of separation of the ions contained in such electrolytes during the isotachophoretic measurement.
  • the electrolyte in the "leading" chamber 12 may be a mixture of hydrochloric acid and aniline, to produce a "leading" chloride ion, while the solution in the "lagging" chamber 11 may be acetic acid, which produces the "lagging" acetate ion.
  • the chloride ion is the first to be separated in the apparatus, while the acetate ion is the last to be separated, as indicated more fully below in connection with FIG. 2.
  • the unitary block 1 further includes a passage 27 communicating with the bottom of the reservoir 12, a damping chamber 4 communicating with the bottom of the channel 27, and a connecting channel 5 which interconnects the damping chamber 4 with one end of a capillary 8.
  • the unitary block 1 includes a connecting channel 6 that provides communication between the bottom of the chamber 11 and the other end of the capillary 8.
  • the unitary block 1 is provided with still-further passages, including channel 29 extending from an exterior surface of the block 1 to the connecting channel 6 for injecting a test sample from a source 31 into the capillary 8.
  • Such channel 29 may advantageously be provided with a sieve 7, as shown.
  • a pair of oppositely disposed input and output ports 3 and 10 are integrally formed in the body 1 for initially loading the capillary 8 with a charge of the leading electrolyte.
  • the port 3 communicates with the damping chamber 4 via a one-way valve 2, while the outlet port 10 communicates with the connection channel 6 via a three-way valve 9.
  • the capillary 8 is formed as a flat groove within the body 1, and is defined between upper and lower parallel boundary walls 33 and 34.
  • the upper wall 33 is a recessed surface of the body 1, while the lower wall 34, like the upper wall 33, may be a surface established within the body 1; alternatively, the wall 34 may be an upper surface of a packing plate 15 supported on top of a separate insulating body 16 that is affixed to opposed lower ends of the body 1 by means of screws 17, 17.
  • the longitudinal path of the capillary 8 between the connection channels 5 and 6 may follow a linear course; alternatively, if additional length of the capillary is desired, the longitudinal axis of the capillary may follow a sinuous or spiral path, as desired. In any case, the planar profile of the capillary 8 is maintained.
  • a semi-permeable membrane 13 may be disposed in the channel 27 interconnecting the bottom of the chamber 12 with the damping chamber 4.
  • a pair of electrodes 14, 14 terminate a corresponding pair of passages 20, 20 extending through the body 1 and into the capillary 8 intermediate its ends.
  • the electrodes 14 are coupled to a suitable recording device 36 for generating an isotachophoregram of the type shown in FIG. 2.
  • the leading electrolyte which as noted before may be a mixture of hydrochloric acid and aniline, is initially introduced into the capillary 8 by means of the inlet port 3, the dotted line position of the valve 2, the damping chamber 4 and the connection channel 5.
  • the residual electrolyte exits via the outlet port 10, the dotted line position of the valve 9 and the connection channel 6.
  • valves 2 and 9 are then adjusted into their solid-line positions shown in FIG. 1, thereby affording communication, in a unitary, fixed and dimensionally stable manner, between the electrodes 18 and 19 via the chamber 11, the connection channel 6, the capillary 8, the connection the 5, the damping chamber 4, the channel 27 and the channel 12.
  • the test sample to be measured is introduced into the connection channel 6 from the source 31.
  • the ions in the resulting solution within the capillary 8 start to migrate in succession past the detecting arrangement 14, 20, with the "leading" chloride ion being detected first and the "lagging" acetate ion being detected last.
  • the various ions in the test sample itself are separated to flow successively past the measuring points, whereby the detecting means 14, 20 develop an appropriate potential for application to the recording device 32.
  • test sample is a nickel plating bath which contains lactate, phosphate, phosphite and hypophosphite ions
  • various ions are separated in the resulting isotachophoregram in the manner shown in FIG. 2.
  • an oxylate ion has been added to the test solution.
  • the entire test interval, from the detection of the leading chloride ion to the detection of the lagging acetate ion was less than 5 minutes, as compared to the normal test interval of 30-100 minutes, exhibited by typical isotachophoretic columns of the prior art.
  • the isolation of the various test and standardization ions takes place in the improved arrangement in even less time, occupying only the last minute of the 5 minute test interval.
  • the voltage applied to the electrodes 18 and 19 from the source 26 is in the range of 4-10 Kv, which is suitable to establish a stabilized current through the column of about 200 microamps.
  • the "leading" electrolyte in the chamber 12 may be present in a concentration of 0.0066 M of HCl and 0.0085 M aniline, while the “lagging" electrolyte in the chamber 11 may be present in a concentration of 0.012 M of acetic acid.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
US05/606,574 1974-08-21 1975-08-21 Isotachophoretic columns Expired - Lifetime US3998719A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CS7400005797A CS178550B1 (en) 1974-08-21 1974-08-21 Isotachophoretic column
CS5797-74 1974-08-21

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US3998719A true US3998719A (en) 1976-12-21

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US (1) US3998719A (hu)
JP (1) JPS5145593A (hu)
CS (1) CS178550B1 (hu)
DE (1) DE2536080C3 (hu)
DK (1) DK368375A (hu)
HU (1) HU173046B (hu)
IT (1) IT1041898B (hu)
NL (1) NL7509814A (hu)
SE (1) SE7509031L (hu)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2468120A1 (fr) * 1979-10-17 1981-04-30 Inst Nat Sante Rech Med Cellule de mesure et dispositif automatique de microelectrophorese analytique
US4459198A (en) * 1981-07-27 1984-07-10 Shimadzu Corporation Electrophoretic apparatus
US4515676A (en) * 1982-12-10 1985-05-07 Kureha Kagaku Kogyo Kabushiki Kaisha Cell unit for observing electrophoresis
US4617104A (en) * 1982-12-29 1986-10-14 Kureha Kagaku Kogyo Kabushiki Kaisha Cell unit for observing electrophoresis
DE3939858A1 (de) * 1988-12-02 1990-06-07 Bio Rad Laboratories Vorrichtung zur kapillarelektrophorese
US5223114A (en) * 1987-06-17 1993-06-29 Board Of Trustees Of The Leland Stanford Junior University On-column conductivity detector for microcolumn electrokinetic separations
US5302264A (en) * 1992-09-02 1994-04-12 Scientronix, Inc. Capillary eletrophoresis method and apparatus
WO1995021382A2 (en) * 1994-02-01 1995-08-10 Fields Robert E Molecular analyzer and method of use
US5840573A (en) * 1994-02-01 1998-11-24 Fields; Robert E. Molecular analyzer and method of use
US20030201179A1 (en) * 1999-10-15 2003-10-30 James Palmer Method for injection and stacking of analytes in high-conductivity samples

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51161886U (hu) * 1975-06-18 1976-12-23
JPS5739788Y2 (hu) * 1977-07-27 1982-09-01
JPS5820926Y2 (ja) * 1977-09-20 1983-05-02 株式会社島津製作所 細管式等速電気泳動装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3649499A (en) * 1968-03-27 1972-03-14 Rauno Erkki Virtanen Method for establishing the zones occurring in electrophoresis and for their quantitative determination
US3705845A (en) * 1970-06-02 1972-12-12 Lkb Produkter Ab Method in counterflow isotachophoresis
US3869365A (en) * 1972-12-19 1975-03-04 Lkb Produkter Ab Method in counter flow isotachophoresis

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3649499A (en) * 1968-03-27 1972-03-14 Rauno Erkki Virtanen Method for establishing the zones occurring in electrophoresis and for their quantitative determination
US3705845A (en) * 1970-06-02 1972-12-12 Lkb Produkter Ab Method in counterflow isotachophoresis
US3869365A (en) * 1972-12-19 1975-03-04 Lkb Produkter Ab Method in counter flow isotachophoresis

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2468120A1 (fr) * 1979-10-17 1981-04-30 Inst Nat Sante Rech Med Cellule de mesure et dispositif automatique de microelectrophorese analytique
US4459198A (en) * 1981-07-27 1984-07-10 Shimadzu Corporation Electrophoretic apparatus
US4515676A (en) * 1982-12-10 1985-05-07 Kureha Kagaku Kogyo Kabushiki Kaisha Cell unit for observing electrophoresis
US4617104A (en) * 1982-12-29 1986-10-14 Kureha Kagaku Kogyo Kabushiki Kaisha Cell unit for observing electrophoresis
US5223114A (en) * 1987-06-17 1993-06-29 Board Of Trustees Of The Leland Stanford Junior University On-column conductivity detector for microcolumn electrokinetic separations
DE3939858A1 (de) * 1988-12-02 1990-06-07 Bio Rad Laboratories Vorrichtung zur kapillarelektrophorese
US5302264A (en) * 1992-09-02 1994-04-12 Scientronix, Inc. Capillary eletrophoresis method and apparatus
WO1995021382A2 (en) * 1994-02-01 1995-08-10 Fields Robert E Molecular analyzer and method of use
WO1995021382A3 (en) * 1994-02-01 1995-11-09 Robert E Fields Molecular analyzer and method of use
US5840573A (en) * 1994-02-01 1998-11-24 Fields; Robert E. Molecular analyzer and method of use
AU699986B2 (en) * 1994-02-01 1998-12-17 Igene Inc. Molecular analyzer and method of use
US20030201179A1 (en) * 1999-10-15 2003-10-30 James Palmer Method for injection and stacking of analytes in high-conductivity samples

Also Published As

Publication number Publication date
DE2536080C3 (de) 1980-09-11
DK368375A (da) 1976-02-22
NL7509814A (nl) 1976-02-24
JPS5145593A (hu) 1976-04-19
IT1041898B (it) 1980-01-10
DE2536080A1 (de) 1976-03-04
HU173046B (hu) 1979-02-28
CS178550B1 (en) 1977-10-31
SE7509031L (sv) 1976-02-23
DE2536080B2 (de) 1980-01-10

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